CN103897685B - 低浓度羧甲基交联剂及制备方法 - Google Patents
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Abstract
本发明涉及一种低浓度羧甲基交联剂及制备方法;由如下化学原料按重量份配比:水100~300份、乙醇130~200份、乳酸锆200~320份、无机碱10~20份、膦基羧酸稳定剂100~130份、有机胺30~100份、异丙醇10~30份;取上述化工原料总计在580~1100份之间任意值配比;将乳酸锆加到含量为80%的乙醇溶液中,加入膦基羧酸稳定剂,保持温度在45℃,加入含量为80%的三乙醇胺;混合物加热到60℃;然后用氢氧化钠水溶液和异丙醇中和到pH8;把混合物加热到80℃,用水搅拌;得到透明的淡黄色的交联剂;本交联剂具有延迟交联、耐高温、性能稳定、低浓度的特性。
Description
技术领域
本发明涉及一种用于气井改造中的压裂过程中使用的交联剂,特别是一种低浓度羧甲基交联剂及制备方法,适合在气井压裂改造过程中携带支撑剂。
背景技术
目前油田上压裂技术是常规的增产技术,是将储层压出人工裂缝,用压裂液携带一定浓度的支撑剂,铺置于人工裂缝中以提高储层的导流能力,从而达到增产的效果。稠化剂作为水基压裂液的主剂,用以提高压裂液的粘度,降低压裂液滤失,悬浮和携带支撑剂。
目前油田上压裂使用的交联剂主要是有机硼交联剂,与羟丙基瓜尔胶水溶液进行交联,普遍存在如下的缺点:
1、由于受羟丙基瓜尔胶的改性程度限制,以其为稠化剂的压裂液体系破胶残渣含量高,一般在350mg/L以上。
2、羟丙基瓜尔胶体系稠化剂与有机硼交联剂存在反胶现象,破胶不彻底,残胶含量高。
两方面因素导致上述压裂液在压裂改造后对储层造成较大的伤害,影响改造效果。
发明内容
本发明的目的是提供一种具有延迟交联特性、耐高温特性、性能稳定的低浓度(稠化剂浓度为0.28%)羧甲基交联剂及制备方法。
本发明所述的一种低浓度羧甲基交联剂,其特征是:包括如下化学原料按重量份配比:
取上述化工原料总计在580~1100份之间任意值配比。
上述涉及到的化学物质其中膦基羧酸稳定剂、乳酸锆为庆阳长庆井下助剂有限责任公司生产,有机胺为一乙醇胺、三乙醇胺、四乙二胺。
无机碱为碳酸钠、氢氧化钠、氢氧化钾等。
低浓度羧甲基交联剂制备方法:
在带有温度计、滴液漏斗和回流装置的四颈圆底烧瓶中,加入200-320克乳酸锆到含量为80%的130-200克乙醇溶液中,在高速搅拌状态下逐渐加入100-130克膦基羧酸稳定剂,缓慢放热,保持温度在45℃以上,在搅拌下加入30-100克含量为80%的三乙醇胺;混合物加热到60℃,恒温4小时,加完继续搅拌1小时;然后用10-20克氢氧化钠水溶液和10-30克异丙醇中和到pH8以上;接着把混合物加热到80℃,恒温4小时,用100-300ml水搅拌;可以得到透明的淡黄色的JL-11交联剂。发明效果
1、交联延迟时间可控。使用本品交联剂,在低浓度羧甲基瓜尔胶水溶液的pH值控制在9以上的情况下,通过调整交联剂的比例,可将液体的初始交联时间控制在1分钟以内,完全交联时间控制在2~5分钟以内。
2、交联冻胶具有较好的耐温耐剪切性能。使用本品交联剂所形成的冻胶,耐温性能可达140℃以上。从图1中可以看出,在170s-1的剪切下,随着温度的逐步升高,粘度缓慢下降,当温度达到149℃时,该液体的粘度仍有55mPa·s。使用本品交联剂的最佳剂量(0.2%)时,液体性能耐温性能良好、稳定;在90℃下,170s-1的剪切速率下剪切1小时,液体粘度仍在200mPa·s以上,远远高于行业标准要求的50mPa·s。
附图说明
图1是冻胶粘度随着温度的逐渐升高而缓慢下降示意图;
图2是冻胶随着温度的升高而粘度快速下降示意图。
具体实施方式
实施例1
低浓度羧甲基交联剂制备方法:
在1000ml带有温度计、滴液漏斗和回流装置的四颈圆底烧瓶中,加入320克乳酸锆到含量为80%的200克乙醇溶液中,在高速搅拌状态下逐渐加入130克膦基羧酸稳定剂,缓慢放热,保持温度在45℃以上,在搅拌下加入100克含量为80%的三乙醇胺;混合物加热到60℃,恒温4小时,加完继续搅拌1小时;然后用20克氢氧化钠水溶液和30异丙醇中和到pH8以上;接着把混合物加热到80℃,恒温4小时,用200ml水搅拌;可以得到透明的淡黄色的JL-11交联剂。该产物可以作为羧甲基羟丙基瓜尔胶压裂液的交联剂。
实施例2
低浓度羧甲基交联剂制备方法:
在1000ml带有温度计、滴液漏斗和回流装置的四颈圆底烧瓶中,加入200克乳酸锆到含量为80%的130克乙醇溶液中,在高速搅拌状态下逐渐加入100克膦基羧酸稳定剂,缓慢放热,保持温度在45℃以上,在搅拌下加入30克含量为80%的三乙醇胺;混合物加热到60℃,恒温4小时,加完继续搅拌1小时;然后用10克氢氧化钠水溶液和10异丙醇中和到pH8以上;接着把混合物加热到80℃,恒温4小时,用150ml水搅拌;可以得到透明的淡黄色的JL-11交联剂。该产物可以作为羧甲基羟丙基瓜尔胶压裂液的交联剂。
实施例中也可通过更换有机胺(一乙醇胺、三乙醇胺、四乙二胺)和无机碱(碳酸钠、氢氧化钠、氢氧化钾)得到透明的淡黄色的JL-11交联剂。
化学反应工艺步骤为:按照上述化学反应配比范围取其值(这里主要提出一个反应流程),在常压下,选择三乙醇胺(或一乙醇胺、四乙二胺等)作为锆离子的配体,多齿配体化合物四乙二胺可以从专业试剂商店购买,也可以由乙二胺和环氧丙烷合成,也可以由乙二胺和氯乙醇在碱性条件下合成。选择乳酸锆的乙醇溶液作为锆离子的来源。
性能评价
基液配方:0.28%CJ2-11稠化剂+0.5%CF-11助排剂+0.50%LF-11粘土稳定剂+0.05%CJSJ-3杀菌剂+0.4%~0.5%CJ-11(s)交联促进剂交联剂:JL-11交联剂
交联比:100:0.2~0.3
从图1中可以看出,冻胶粘度随着温度的逐渐升高而缓慢下降,当温度为149℃时,粘度保持在55mPa·s。
在过交联的情况下,常温状态的冻胶挑挂性好,冻胶强度大,但是从上图2中可以看出,冻胶随着温度的升高而粘度快速下降;剪切9min,温度88℃时,粘度从开始时的750mPa·s下降到50mPa·s。
降低压裂液中聚合物用量既可以减少浓缩胶的数量,也可以减少浓缩胶中存在的水不溶物,有利于形成更清洁的和高导流的支撑裂缝。
Claims (2)
1.一种低浓度羧甲基交联剂,其特征是:由如下化学原料按重量份配比:
取上述化工原料总计在580~1100份之间任意值配比;
所述的有机胺为一乙醇胺、三乙醇胺;
所述的无机碱为碳酸钠、氢氧化钠、氢氧化钾。
2.一种权利要求1所述的低浓度羧甲基交联剂制备方法;其特征在于:
在带有温度计、滴液漏斗和回流装置的四颈圆底烧瓶中,加入200-320克乳酸锆到含量为80%的130-200克乙醇溶液中,在高速搅拌状态下逐渐加入100-130克膦基羧酸稳定剂,缓慢放热,保持温度在45℃,在搅拌下加入30-100克含量为80%的三乙醇胺;混合物加热到60℃,恒温4小时,加完继续搅拌1小时;然后用10-20克氢氧化钠水溶液和10-30克异丙醇中和到pH8;接着把混合物加热到80℃,恒温4小时,用100-300ml水搅拌;得到透明的淡黄色的交联剂。
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CN101688112A (zh) * | 2007-05-11 | 2010-03-31 | 普拉德研究及开发股份有限公司 | 用络合的金属交联剂进行油井处理 |
CN101649194A (zh) * | 2009-09-15 | 2010-02-17 | 克拉玛依市正诚有限公司 | 复合多价金属离子交联剂及其生产方法和使用方法 |
CN102134481B (zh) * | 2011-01-18 | 2013-05-22 | 大庆油田有限责任公司 | 羧甲基羟丙基胍胶水基压裂液 |
CN102492413A (zh) * | 2011-12-05 | 2012-06-13 | 北京希涛技术开发有限公司 | 甲醇基压裂液可控交联剂的开发 |
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